Diflukortolon valerat ve klorkinaldol'ün farmasötik preparatlarda spektrofotometrik yöntemlerle aynı anda miktar tayinleri
Özet
143SUMMARYSimultaneous spectrophotometric determination of diflucortolone valerate andchlorquinaldol in pharmaceutical preparationsIn this thesis; our aim was to develop new methods for the simultaneousdetermination of diflucortolone valerate (DİF) and chlorquinaldol (KLO) in theirbinary mixtures. For this reason we selected the spectrophotometric methods andratio spectra first derivative spectrophotometry (1DD) and Principle ComponentRegression (PCR) technique were used for this purpose. In 1DD; analytical signalswere measured at 238.1 nm for DİF and at 269.7 nm for KLO in the first derivativespectra of the ratio spectra obtained by dividing the UV spectra of the mixture ofDİF + KLO in methanol-water (3:1) in the range 200-350 nm (Πλ = 2 nm) using thespectra of 9.6 μg/mL solution of DİF in methanol-water (3:1) and 4.0 μg/mLsolution of KLO in methanol-water (3:1) as divisor. In PCR technique; Absorbancesof the mixture solutions of DİF and KLO in methanol-water (3:1) were measured at60 wavelengths in the range 230-340 nm as Πλ = 2 and their analysis were made byPCR method. Mean recoveries and the standard deviations of the methods werefound as % 99.86 and % 1.98 in 1DD and % 100.29 and % 1.48 in PCR method forDİF and, % 100.29 and % 1.64 in 1DD and % 100.05 and % 0.64 in PCR methodfor KLO, respectively. Working range were found as 0.88-3.00 μg/mL for DİFand 1.00-11.20 μg/mL for KLO in 1DD and in PCR method. Developedspectrophotometric methods were successfully applied to cream formulationsmarketed in Turkey. In addition we developed a HPLC method in which ACE C18reverse phase column and methanol-phosphate buffer (pH : 5.5, 0.1 M) (95:5 v/v)mobil phase was used and 220 nm was selected for detection. Ephedrinehydrochloride was used as internal standard. Retention times were 2.54 min. forephedrine hydrochloride, 3.44 min. for DİF and 4.46 min. for KLO. In HPLCmethod, working range was found as 2.40-300.00 μg/mL for DİF and 0.72 -240.00 μg/mL for KLO. HPLC method was also applied to the same selectedformulations and the results were compared with each other statistically. It was144concluded that these three methods developed could be used for the routine analysisof the cream formulations containing these drugs.Keywords: Chlorquinaldol; Diflucortolone valerate; Liquid chromatography;Principal component regression; Pharmaceutical preparation; Ratio spectraderivative spectrophotometry.